CN103498074A - Novel Ni3Al-based self-lubricating composite material and preparing method thereof - Google Patents

Novel Ni3Al-based self-lubricating composite material and preparing method thereof Download PDF

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Publication number
CN103498074A
CN103498074A CN201310494301.XA CN201310494301A CN103498074A CN 103498074 A CN103498074 A CN 103498074A CN 201310494301 A CN201310494301 A CN 201310494301A CN 103498074 A CN103498074 A CN 103498074A
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powder
novel
self
lubricating composite
composite material
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史晓亮
翟文正
薛冰
徐增师
姚杰
宋思远
陈龙
朱庆帅
肖业成
章桥新
王玉伏
冯四平
张崧
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Wuhan University of Technology WUT
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Abstract

The invention provides a novel Ni3Al-based self-lubricating composite material and a preparing method thereof. The self-lubricating composite material is made of Ni powder, Al powder and a graphenenanosheet. The molar ratio of Ni to Al is 4.5 to 1, and the graphene nanosheet accounts, by weight, 0.5-1.5% of the total mass of the Ni powder and the Al powder. A Ni3Al intermetallic compound serves as a matrix of the self-lubricating composite material, the graphene nanosheet serves as a lubricating phase and a reinforced phase, the Ni3Al-based self-lubricating composite material is prepared through spark plasma sintering, and the combination of the matrix of the prepared self-lubricating composite material and the interface of the graphene nanosheet is good. Besides, by means of the spark plasma sintering technology, the novel Ni3Al-based self-lubricating composite material taking the graphene nanosheet as the lubricating phase and the reinforced phase is high in purity and good in compactness, and has good tribology performance. In the preparing process, related steps are simple and convenient to achieve, and the method is suitable for large-scale production.

Description

A kind of novel Ni 3al based self lubricated composite material and preparation method thereof
Technical field
The present invention relates to a kind of novel Ni of graphene nanometer sheet as lubricated phase of take 3al based self lubricated composite material and preparation method thereof.
Background technology
Ni 3al base alloy has many good performances, comprises high-melting-point, high resistance to high temperature oxidation, corrosion-resistant, higher hot strength and creep resistance and high specific tenacity, and has the positive temperature effect of peak temperature with lower yield strength.Just because of these good characteristics, Ni 3al base alloy as high-temperature structural material in civilian and military industry, have a extensive future ([1] Chen Jin smoke tree, Zhu Dingyi, Lin Dengyi. Ni 3the advances and application of Al base alloy. material Leader, 2006 (20): 35-38.).
Relevant Ni 3the research that Al intermetallic compound and tungstate, hard particles etc. prepare high temperature high abrasion matrix material by powder metallurgic method also has report ([2] Shengyu Zhu, Qinling Bi, Jun Yang, Weimin Liu. Ni recently 3al Matrix Composite with Lubricious Tungstate at High Temperatures. Tribol Lett, 2012 (45): 251-255; [3] Karin Gong, Heli Luo, Di Feng, Changhai Li. Wear of Ni 3al-based materials and its chromium-carbide reinforced composites. Wear, 2008 (265): 1751-1755.).In order to improve Ni 3the tribological property of Al based composites, Chinese scholars has been carried out a large amount of research work.Research has in the past improved Ni to a great extent 3the tribological property of Al based self lubricated composite material, and energy-conservation of consumption reduction, fall oligosaprobic trend new matrix material is had higher requirement, for this reason, scholars are still constantly seeking better lubricated phase, this class is lubricated not only possesses good frictional coefficient and wear rate mutually, and can reduce pollution.
Summary of the invention
The object of the present invention is to provide a kind of novel Ni 3al based self lubricated composite material and preparation method thereof, this self-lubricating composite is compounded in Ni by the graphene nanometer sheet original position 3in the Al matrix, the matrix material of gained has excellent tribological property, and the preparation method is simple and easy to realization, and in preparation process, processing parameter is easily controlled.
For the object of the invention is achieved, therefore the technical scheme of taking is:
A kind of novel Ni 3the Al self-lubricating composite, it is prepared from by Ni powder, Al powder and graphene nanometer sheet, mol ratio=4.5:1 of Ni:Al wherein, the 0.5-1.5% that the quality of graphene nanometer sheet is Ni powder, Al powder total mass.
A kind of novel Ni 3the preparation method of Al self-lubricating composite, it comprises the steps:
1) press mol ratio=4.5:1 of Ni:Al, choose Ni powder, Al powder; Account for the 0.5-1.5% of Ni powder, Al powder total mass by graphene nanometer sheet, choose graphene nanometer sheet, Ni powder, Al powder and graphene nanometer sheet are mixed, prepared burden;
2) above-mentioned batching is placed in vibromill and dry grinds, obtain mixed powder;
3) mixed powder is adopted discharge plasma sintering obtain described novel Ni 3the Al self-lubricating composite.
In such scheme, the Ni powder in described step 1) or the median size of Al powder are the 30-50 micron.
In such scheme, the graphene nanometer sheet thickness in described step 1) is 20 nanometers-2 micron, and particle diameter is the 5-200 micron.
The inwall of the ball grinder in the vibromill in such scheme, described step 2) is tetrafluoroethylene, and vibrational frequency is 45Hz, and amplitude is 5mm, and vibration force is 10000N, and duration of oscillation is 20-40 minute.
In such scheme, the described discharge plasma sintering process of described step 3) is: sintering temperature is that 1130-1140 ℃, temperature rise rate are that 100-130 ℃/min, sintering pressure are that 40-70MPa, vacuum tightness are 1 * 10 -2-1 * 10 -1pa, soaking time are 5-12min.
The invention has the beneficial effects as follows:
1, preparation process is convenient, fast: adopt vibratory milling in the presintering powder preparation process, period of oscillation is short.
2, simple to operate, feasibility is high: sintering process adopts SPS to carry out the sintering of material, and the sintering reaction cycle is short, process stabilizing, and the self-lubricating composite purity of preparation is high.
3, prepare required equipment simple: have raw material sources extensively, price is lower, equipment cost is lower, hold manageable characteristics, and is applicable to large-scale production.
4, adopt SPS to prepare self-lubricating composite, reduced sintering temperature, shortened sintering time, save energy, the complex phase generation because adding graphene nanometer sheet to cause that reduces synthetic cost and avoided to the full extent.
5, a kind of novel Ni that prepared by the present invention 3the Al based self lubricated composite material has good tribological property.
In sum, the present invention chooses Ni 3the Al intermetallic compound is as the matrix of self-lubricating composite, and graphene nanometer sheet is mutually lubricated and wild phase, adopts a kind of novel Ni of discharge plasma sintering 3the Al based self lubricated composite material, the matrix of the self-lubricating composite of preparation is combined well with the graphene nanometer sheet interface.In addition, this employing discharge plasma sintering technique prepares the novel Ni of graphene nanometer sheet for mutually lubricated and wild phase 3the Al based self lubricated composite material, its purity is high, compactness good, and has good tribological property.Step method related in preparation process is simple and convenient, is applicable to the mass-producing batch production.
The accompanying drawing explanation
Fig. 1 is preparation technology's schema of the present invention.
Fig. 2 is the present invention's graphene nano film studio emission surface sweeping electromicroscopic photograph used.
Fig. 3 is the present invention's graphene nano film studio emission surface sweeping electromicroscopic photograph used.
Fig. 4 is the novel Ni of the embodiment of the present invention 1 preparation 3the fracture field emission surface sweeping electromicroscopic photograph of Al based self lubricated composite material.
Fig. 5 is the novel Ni that the embodiment of the present invention 1 makes 3the electronic probe photo of Al based self lubricated composite material frictional abrasion surface.
Fig. 6 is the novel Ni that the embodiment of the present invention 2 makes 3the field emission scanning electron microscope photo of Al based self lubricated composite material frictional abrasion surface fracture.
Fig. 7 to Fig. 9 is respectively under room temperature condition, the obtained novel Ni of the test embodiment of the present invention 1,2,3 3the frictional coefficient curve of Al based self lubricated composite material.
Figure 10 is under room temperature condition, the prepared novel Ni of the test embodiment of the present invention 1,2,3 3the wear rate figure of Al based self lubricated composite material, test condition is: load 15N, sliding velocity 0.45m/s, time 40min, friction radius 3.5mm.
Embodiment
Below in conjunction with drawings and Examples, further the present invention will be described, but content of the present invention not only is confined to the following examples.
embodiment 1:
As shown in Figure 1, the present embodiment provides a kind of novel Ni 3the preparation method of Al based self lubricated composite material, it comprises the steps:
1) take Ni powder, Al powder is initial feed, and graphene nanometer sheet is lubricant, presses mol ratio=4.5:1 of Ni:Al, takes 9.5424 gram Ni powder, 0.9720 gram Al powder, amounts to 10.5144g, mixes, and obtains mixed powder; Then add the 0.0526g graphene nanometer sheet in above-mentioned mixed powder, prepared burden (admixtion);
2) above-mentioned batching is placed in vibromill and dry grinds, vibrating ball grinding jar inwall is tetrafluoroethylene, and vibrational frequency is 45Hz, and amplitude is 5mm, and vibration force is 10000N, and power is 0.75 kilowatt, and duration of oscillation is 20 minutes, obtains mixed powder;
3) adopt discharge plasma sintering to obtain described novel Ni above-mentioned mixed powder 3the Al self-lubricating composite.Discharge plasma sintering process is: sintering temperature is that 1130 ℃, temperature rise rate are that 100 ℃/min, sintering pressure are that 40MPa, vacuum tightness are 1 * 10 -2pa, soaking time are 5min, after sintering, obtain a kind of novel Ni that comprises graphene nanometer sheet 3the Al based self lubricated composite material.
Fig. 2 and Fig. 3 are the FESEM pictures of the graphene nanometer sheet used in embodiment; Fig. 4 is the prepared novel Ni of embodiment 1 3the FESEM photo of Al based self lubricated composite material fracture.Fig. 2 and Fig. 3 show that there is fold in the graphene nanometer sheet surface, and the sharpness of border of graphene nanometer sheet, and transparency is high between layers, show that graphene nanometer sheet consists of multi-layer graphene; Fig. 4 shows that the self-lubricating composite density that embodiment 1 prepares is high, and graphene nanometer sheet is embedded in matrix, with basal body interface, is combined well, and good interface is in conjunction with guaranteeing novel Ni 3the Al based self lubricated composite material possesses excellent over-all properties.Adopt the prepared novel Ni of HVS-1000 type digital display microhardness instrument test implementation example 1 3the hardness of Al based self lubricated composite material is 7.95GPa, and relative density is 99.2%.Fig. 5 is the obtained novel Ni of embodiment 1 3the electronic probe photo that the Al based self lubricated composite material is frictional abrasion surface under the 15N condition in load, Fig. 5 illustrates that this matrix material frictional abrasion surface is smooth, guarantees that it has good tribological property.Fig. 7 and Figure 10 illustrate the frictional coefficient of this self-lubricating composite little (approximately 0.22) and fluctuating range less, wear rate is 7.7 * 10 -5mm 3/ (Nm), embody good tribological property.
embodiment 2:
The present embodiment provides a kind of novel Ni 3the preparation method of Al based self lubricated composite material, it comprises the steps:
1) take Ni powder, Al powder is initial feed, and graphene nanometer sheet is lubricant, presses mol ratio=4.5:1 of Ni:Al, takes 9.5424 gram Ni powder, 0.9720 gram Al powder, amounts to 10.5144g, mixes, and obtains mixed powder; Then add the 0.1051g graphene nanometer sheet in above-mentioned mixed powder, prepared burden (admixtion);
2) above-mentioned batching is placed in vibromill and dry grinds, vibrating ball grinding jar inwall is tetrafluoroethylene, and vibrational frequency is 45Hz, and amplitude is 5mm, and vibration force is 10000N, and power is 0.75 kilowatt, and duration of oscillation is 30 minutes, obtains mixed powder;
3) adopt discharge plasma sintering to obtain described a kind of novel Ni above-mentioned mixed powder 3the Al self-lubricating composite.Discharge plasma sintering process is: sintering temperature is that 1135 ℃, temperature rise rate are that 115 ℃/min, sintering pressure are that 55MPa, vacuum tightness are 4.5 * 10 -2pa, soaking time are 8min, after sintering, obtain a kind of novel Ni that comprises graphene nanometer sheet 3the Al based self lubricated composite material.
Adopt the prepared novel Ni of HVS-1000 type digital display microhardness instrument test implementation example 2 3the hardness of Al based self lubricated composite material is 8.25GPa, and relative density is 99.1%.Fig. 6 is the novel Ni that embodiment 2 makes 3the field emission scanning electron microscope photo of Al based self lubricated composite material frictional abrasion surface fracture.Fig. 6 has shown the zone that has produced two kinds of various grain sizes on the inferior surface of frictional wear.The zone near frictional abrasion surface is the superfine crystal particle district, away from frictional abrasion surface, is the large die region with clear crystal boundary.The people such as Prasad study and find that the superfine crystal particle structure that is in the frictional abrasion surface below can cause high friction to change ([8] S.V. Prasad to low friction, C.C. Battaile, P.G. Kotula. Friction transitions in nanocrystalline nickel. Scripta Mater, 2011 (64): 729-732.).Novel Ni 3the inferior surface of the frictional wear of Al based self lubricated composite material produces the superfine crystal particle district, shows that it has good tribological property.Fig. 8 and Figure 10 illustrate the frictional coefficient of this self-lubricating composite little (approximately 0.22) and fluctuating range little, wear rate is 6.5 * 10 -5mm 3/ (Nm), embody good tribological property.
embodiment 3:
The present embodiment provides a kind of novel Ni 3the preparation method of Al based self lubricated composite material, it comprises the steps:
1) take Ni powder, Al powder is initial feed, and graphene nanometer sheet is lubricant, presses mol ratio=4.5:1 of Ni:Al, takes 9.5424 gram Ni powder, 0.9720 gram Al powder, amounts to 10.5144g, mixes, and obtains mixed powder; Then add the 0.1577g graphene nanometer sheet in above-mentioned mixed powder, prepared burden (admixtion);
2) above-mentioned batching is placed in vibromill and dry grinds, vibrating ball grinding jar inwall is tetrafluoroethylene, and vibrational frequency is 45Hz, and amplitude is 5mm, and vibration force is 10000N, and power is 0.75 kilowatt, and duration of oscillation is 40 minutes, obtains mixed powder;
3) adopt discharge plasma sintering to obtain described a kind of novel Ni above-mentioned mixed powder 3the Al self-lubricating composite.Discharge plasma sintering process is: sintering temperature is that 1140 ℃, temperature rise rate are that 130 ℃/min, sintering pressure are that 70MPa, vacuum tightness are 1 * 10 -1pa, soaking time are 12min, after sintering, obtain a kind of novel Ni that comprises graphene nanometer sheet 3the Al based self lubricated composite material.
The prepared novel Ni by HVS-1000 type digital display microhardness instrument test implementation example 3 3the hardness of Al based self lubricated composite material is 8.12GPa, and relative density is 98.9%.Fig. 9 is under room temperature condition, the prepared novel Ni of the test embodiment of the present invention 3 3the frictional coefficient curve of Al based self lubricated composite material, test condition is: load 15N, sliding velocity 0.45m/s, time 40min, friction radius 3.5mm.Fig. 9 illustrate the frictional coefficient of this self-lubricating composite little (approximately 0.21) and fluctuating range little.In addition, Figure 10 shows the novel Ni that embodiment 3 prepares 3the wear rate of Al based self lubricated composite material is 7.6 * 10 -5mm 3/ (Nm).Novel Ni 3the Al based self lubricated composite material has shown good tribological property.
Each cited raw material of the present invention can be realized the present invention, and the bound value of each raw material, interval value can realize the present invention, bound value and the interval value of processing parameter of the present invention (as frequency, temperature, time, vacuum tightness etc.) can be realized the present invention, at this, do not enumerate embodiment.

Claims (6)

1. a novel Ni 3the Al self-lubricating composite, is characterized in that, it is prepared from by Ni powder, Al powder and graphene nanometer sheet, mol ratio=4.5:1 of Ni:Al wherein, the 0.5-1.5% that the quality of graphene nanometer sheet is Ni powder, Al powder total mass.
2. a novel Ni 3the preparation method of Al self-lubricating composite, is characterized in that it comprises the steps:
1) press mol ratio=4.5:1 of Ni:Al, choose Ni powder, Al powder; Account for the 0.5-1.5% of Ni powder, Al powder total mass by graphene nanometer sheet, choose graphene nanometer sheet, Ni powder, Al powder and graphene nanometer sheet are mixed, prepared burden;
2) above-mentioned batching is placed in vibromill and dry grinds, obtain mixed powder;
3) mixed powder is adopted discharge plasma sintering obtain described novel Ni 3the Al self-lubricating composite.
3. novel Ni as claimed in claim 2 3the preparation method of Al self-lubricating composite, is characterized in that, the Ni powder in described step 1) or the median size of Al powder are the 30-50 micron.
4. novel Ni as claimed in claim 2 3the preparation method of Al self-lubricating composite, is characterized in that, the graphene nanometer sheet thickness in described step 1) is 20 nanometers-2 micron, and particle diameter is the 5-200 micron.
5. novel Ni as claimed in claim 2 3the preparation method of Al self-lubricating composite, is characterized in that, described step 2) in vibromill in the inwall of ball grinder be tetrafluoroethylene, vibrational frequency is 45Hz, amplitude is 5mm, vibration force is 10000N, duration of oscillation is 20-40 minute.
6. novel Ni as claimed in claim 2 3the preparation method of Al self-lubricating composite, is characterized in that, the described discharge plasma sintering process of described step 3) is: sintering temperature is that 1130-1140 ℃, temperature rise rate are that 100-130 ℃/min, sintering pressure are that 40-70MPa, vacuum tightness are 1 * 10 -2-1 * 10 -1pa, soaking time are 5-12min.
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Cited By (11)

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CN103752819A (en) * 2014-02-18 2014-04-30 武汉理工大学 B2 type NiAl-based self-lubricating composite materials and preparing method thereof
CN104762500A (en) * 2014-12-17 2015-07-08 武汉理工大学 Novel Ni3Al-based self-lubricating material with MoO3 plate-shaped crystal as lubricating phase and reinforcing phase, and preparation method thereof
CN105463226A (en) * 2015-12-28 2016-04-06 黄河水利职业技术学院 Modified NiAl-based self-lubricating material and preparation method thereof
CN105603233A (en) * 2016-01-15 2016-05-25 武汉理工大学 Novel NiAl-based self-lubricating material using Ag and Mo-B-O-Si four-element platy crystal as composite lubricating phase and reinforcing phase and preparation method of novel NiAl-based self-lubricating material
CN105950914A (en) * 2016-05-12 2016-09-21 武汉理工大学 Novel Ni3Al based self-lubricating material with hollow spherical powder as lubricating phase and preparation method
CN106834807A (en) * 2016-12-29 2017-06-13 苏州大学 A kind of Graphene enhancing two-phase metal aluminide composite and preparation method thereof
CN106834808A (en) * 2017-02-17 2017-06-13 武汉理工大学 A kind of Ni3Al based self-lubricating materials and preparation method thereof
CN107460375A (en) * 2017-07-21 2017-12-12 天津大学 A kind of method of improvement Ni graphene heteromers reinforced aluminum matrix composites mechanical properties
CN108044092A (en) * 2017-12-13 2018-05-18 柳州璞智科技有限公司 A kind of robot self-lubricating material
CN108531780A (en) * 2018-05-15 2018-09-14 兰州理工大学 A kind of preparation method of graphene enhancing nickel alumin(i)um alloy based composites
CN114293133A (en) * 2021-12-31 2022-04-08 西安交通大学 Spray coating material for forming wide-temperature-range self-lubricating coating by atmospheric plasma spraying, preparation method and application thereof

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CN102634715A (en) * 2012-04-17 2012-08-15 武汉理工大学 Ni3Al intermetallic-based solid self-lubricating composite material and preparation method thereof
CN103334030A (en) * 2013-06-09 2013-10-02 武汉理工大学 Graphene-containing titanium-aluminum-base self-lubricating composite material and preparation method thereof

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CN102634715A (en) * 2012-04-17 2012-08-15 武汉理工大学 Ni3Al intermetallic-based solid self-lubricating composite material and preparation method thereof
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Cited By (16)

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Publication number Priority date Publication date Assignee Title
CN103752819A (en) * 2014-02-18 2014-04-30 武汉理工大学 B2 type NiAl-based self-lubricating composite materials and preparing method thereof
CN104762500A (en) * 2014-12-17 2015-07-08 武汉理工大学 Novel Ni3Al-based self-lubricating material with MoO3 plate-shaped crystal as lubricating phase and reinforcing phase, and preparation method thereof
CN104762500B (en) * 2014-12-17 2016-11-30 武汉理工大学 A kind of with MoO3platelike crystal is lubrication phase and the novel Ni strengthening phase3al based self-lubricating material and preparation method thereof
CN105463226A (en) * 2015-12-28 2016-04-06 黄河水利职业技术学院 Modified NiAl-based self-lubricating material and preparation method thereof
CN105463226B (en) * 2015-12-28 2017-07-28 黄河水利职业技术学院 A kind of modified NiAl based self-lubricating materials and preparation method thereof
CN105603233A (en) * 2016-01-15 2016-05-25 武汉理工大学 Novel NiAl-based self-lubricating material using Ag and Mo-B-O-Si four-element platy crystal as composite lubricating phase and reinforcing phase and preparation method of novel NiAl-based self-lubricating material
CN105603233B (en) * 2016-01-15 2017-05-17 武汉理工大学 NiAl-based self-lubricating material using Ag and Mo-B-O-Si four-element platy crystal as composite lubricating phase and reinforcing phase and preparation method of novel NiAl-based self-lubricating material
CN105950914A (en) * 2016-05-12 2016-09-21 武汉理工大学 Novel Ni3Al based self-lubricating material with hollow spherical powder as lubricating phase and preparation method
CN106834807B (en) * 2016-12-29 2019-02-05 苏州大学 A kind of graphene enhancing two-phase metal aluminide composite material and preparation method
CN106834807A (en) * 2016-12-29 2017-06-13 苏州大学 A kind of Graphene enhancing two-phase metal aluminide composite and preparation method thereof
CN106834808A (en) * 2017-02-17 2017-06-13 武汉理工大学 A kind of Ni3Al based self-lubricating materials and preparation method thereof
CN107460375A (en) * 2017-07-21 2017-12-12 天津大学 A kind of method of improvement Ni graphene heteromers reinforced aluminum matrix composites mechanical properties
CN108044092A (en) * 2017-12-13 2018-05-18 柳州璞智科技有限公司 A kind of robot self-lubricating material
CN108531780A (en) * 2018-05-15 2018-09-14 兰州理工大学 A kind of preparation method of graphene enhancing nickel alumin(i)um alloy based composites
CN114293133A (en) * 2021-12-31 2022-04-08 西安交通大学 Spray coating material for forming wide-temperature-range self-lubricating coating by atmospheric plasma spraying, preparation method and application thereof
CN114293133B (en) * 2021-12-31 2022-11-04 西安交通大学 Spraying material of wide-temperature-range self-lubricating coating, preparation method and application thereof

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